WO2001016966A1 - Dispositif a thermistance - Google Patents
Dispositif a thermistance Download PDFInfo
- Publication number
- WO2001016966A1 WO2001016966A1 PCT/JP2000/005892 JP0005892W WO0116966A1 WO 2001016966 A1 WO2001016966 A1 WO 2001016966A1 JP 0005892 W JP0005892 W JP 0005892W WO 0116966 A1 WO0116966 A1 WO 0116966A1
- Authority
- WO
- WIPO (PCT)
- Prior art keywords
- temperature
- metal oxide
- oxide
- thermistor
- resistance
- Prior art date
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- 229910044991 metal oxide Inorganic materials 0.000 claims abstract description 84
- 150000004706 metal oxides Chemical class 0.000 claims abstract description 84
- 239000000203 mixture Substances 0.000 claims abstract description 78
- 239000002131 composite material Substances 0.000 claims abstract description 45
- 238000002844 melting Methods 0.000 claims abstract description 20
- 230000008018 melting Effects 0.000 claims abstract description 20
- 230000000737 periodic effect Effects 0.000 claims abstract description 8
- 238000002156 mixing Methods 0.000 claims description 65
- 239000002245 particle Substances 0.000 claims description 65
- 238000004519 manufacturing process Methods 0.000 claims description 61
- 239000002994 raw material Substances 0.000 claims description 59
- 238000000034 method Methods 0.000 claims description 44
- 238000010298 pulverizing process Methods 0.000 claims description 24
- 238000010304 firing Methods 0.000 claims description 23
- 229910052751 metal Inorganic materials 0.000 claims description 13
- 239000002184 metal Substances 0.000 claims description 13
- 238000001354 calcination Methods 0.000 claims description 10
- 229910052712 strontium Inorganic materials 0.000 claims description 7
- 229910052692 Dysprosium Inorganic materials 0.000 claims description 6
- 229910052693 Europium Inorganic materials 0.000 claims description 6
- 229910052688 Gadolinium Inorganic materials 0.000 claims description 6
- 229910052689 Holmium Inorganic materials 0.000 claims description 6
- 229910052777 Praseodymium Inorganic materials 0.000 claims description 6
- 229910052772 Samarium Inorganic materials 0.000 claims description 6
- 229910052771 Terbium Inorganic materials 0.000 claims description 6
- 229910052769 Ytterbium Inorganic materials 0.000 claims description 6
- 229910052804 chromium Inorganic materials 0.000 claims description 6
- 229910052749 magnesium Inorganic materials 0.000 claims description 6
- 229910052779 Neodymium Inorganic materials 0.000 claims description 5
- 229910052791 calcium Inorganic materials 0.000 claims description 5
- 229910052758 niobium Inorganic materials 0.000 claims description 5
- 229910052698 phosphorus Inorganic materials 0.000 claims description 5
- 229910052706 scandium Inorganic materials 0.000 claims description 5
- 229910052719 titanium Inorganic materials 0.000 claims description 5
- 229910052727 yttrium Inorganic materials 0.000 claims description 5
- 229910052726 zirconium Inorganic materials 0.000 claims description 5
- 229910052684 Cerium Inorganic materials 0.000 claims description 4
- 229910052742 iron Inorganic materials 0.000 claims description 4
- 229910052748 manganese Inorganic materials 0.000 claims description 4
- 229910052757 nitrogen Inorganic materials 0.000 claims description 4
- 229910052715 tantalum Inorganic materials 0.000 claims description 4
- 229910052691 Erbium Inorganic materials 0.000 claims description 3
- 229910052775 Thulium Inorganic materials 0.000 claims description 3
- 239000000919 ceramic Substances 0.000 claims description 3
- 229910052733 gallium Inorganic materials 0.000 claims description 3
- 229910052741 iridium Inorganic materials 0.000 claims description 3
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 229910052718 tin Inorganic materials 0.000 claims description 3
- 229910052721 tungsten Inorganic materials 0.000 claims description 3
- 229910052720 vanadium Inorganic materials 0.000 claims description 3
- 244000124853 Perilla frutescens Species 0.000 claims description 2
- 229910052788 barium Inorganic materials 0.000 claims description 2
- 229910052796 boron Inorganic materials 0.000 claims description 2
- 229910052732 germanium Inorganic materials 0.000 claims description 2
- 229910052735 hafnium Inorganic materials 0.000 claims description 2
- 229910052750 molybdenum Inorganic materials 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims 1
- 229910052763 palladium Inorganic materials 0.000 claims 1
- 229910052702 rhenium Inorganic materials 0.000 claims 1
- 229910052703 rhodium Inorganic materials 0.000 claims 1
- 229910052707 ruthenium Inorganic materials 0.000 claims 1
- 238000007493 shaping process Methods 0.000 claims 1
- 229910052713 technetium Inorganic materials 0.000 claims 1
- 239000000126 substance Substances 0.000 abstract 1
- 238000002360 preparation method Methods 0.000 description 45
- 230000000694 effects Effects 0.000 description 21
- 239000000843 powder Substances 0.000 description 21
- 239000000463 material Substances 0.000 description 19
- 238000005245 sintering Methods 0.000 description 16
- WABPQHHGFIMREM-UHFFFAOYSA-N lead(0) Chemical compound [Pb] WABPQHHGFIMREM-UHFFFAOYSA-N 0.000 description 14
- 239000002609 medium Substances 0.000 description 14
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- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Substances [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 11
- 238000001035 drying Methods 0.000 description 9
- 239000002689 soil Substances 0.000 description 9
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- 229910052799 carbon Inorganic materials 0.000 description 6
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- 239000011777 magnesium Substances 0.000 description 5
- 238000010586 diagram Methods 0.000 description 4
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- 239000011268 mixed slurry Substances 0.000 description 4
- 229910052697 platinum Inorganic materials 0.000 description 4
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- 239000003795 chemical substances by application Substances 0.000 description 2
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- 238000001514 detection method Methods 0.000 description 2
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- 239000002270 dispersing agent Substances 0.000 description 2
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- 239000012153 distilled water Substances 0.000 description 2
- 238000001704 evaporation Methods 0.000 description 2
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 1
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 description 1
- 229910026161 MgAl2O4 Inorganic materials 0.000 description 1
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
- 241000287463 Phalacrocorax Species 0.000 description 1
- KZNMRPQBBZBTSW-UHFFFAOYSA-N [Au]=O Chemical class [Au]=O KZNMRPQBBZBTSW-UHFFFAOYSA-N 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- KZHJGOXRZJKJNY-UHFFFAOYSA-N dioxosilane;oxo(oxoalumanyloxy)alumane Chemical compound O=[Si]=O.O=[Si]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O.O=[Al]O[Al]=O KZHJGOXRZJKJNY-UHFFFAOYSA-N 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 229910052571 earthenware Inorganic materials 0.000 description 1
- 238000004453 electron probe microanalysis Methods 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910001922 gold oxide Inorganic materials 0.000 description 1
- 229910021478 group 5 element Inorganic materials 0.000 description 1
- 229910021472 group 8 element Inorganic materials 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- GKOZUEZYRPOHIO-UHFFFAOYSA-N iridium atom Chemical compound [Ir] GKOZUEZYRPOHIO-UHFFFAOYSA-N 0.000 description 1
- 238000005304 joining Methods 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 229910052863 mullite Inorganic materials 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 229910052596 spinel Inorganic materials 0.000 description 1
- 230000000087 stabilizing effect Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
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- C01G45/1221—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof
- C01G45/125—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof of the type[MnO3]n-, e.g. Li2MnO3, Li2[MxMn1-xO3], (La,Sr)MnO3
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- C01G45/125—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof of the type[MnO3]n-, e.g. Li2MnO3, Li2[MxMn1-xO3], (La,Sr)MnO3
- C01G45/1264—Manganates or manganites with a manganese oxidation state of Mn(III), Mn(IV) or mixtures thereof of the type[MnO3]n-, e.g. Li2MnO3, Li2[MxMn1-xO3], (La,Sr)MnO3 containing rare earth, e.g. La1-xCaxMnO3, LaMnO3
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- C01G51/56—Cobaltates containing alkali metals, e.g. LiCoO2 containing manganese of the type [MnO3]2-, e.g. Li2[CoxMn1-xO3], Li2[MyCoxMn1-x-yO3
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- C01G53/42—Nickelates containing alkali metals, e.g. LiNiO2
- C01G53/44—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese
- C01G53/56—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese of the type [MnO3]2-, e.g. Li2[NixMn1-xO3], Li2[MyNixMn1-x-yO3
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Definitions
- the present invention can detect temperature over a wide temperature range from a room temperature to a high temperature range of about 1000 ° C., and particularly a wide-range thermistor suitable as a temperature sensor. It relates to a star element and its manufacturing method. Background art
- the thermistor element has the characteristic that its resistance value changes with temperature, and its characteristics are generally represented by the resistance value and the temperature coefficient of resistance (temperature dependence of the resistance value).
- the resistance of the thermal element When used as a temperature sensor, the resistance of the thermal element must correspond to the resistance range of the temperature detection circuit that constitutes the temperature sensor. In this case, it is desirable that the value be in the range of 100 ⁇ to 100 OkQ. Further, when a thermal history is given to the thermistor element, it is required that the resistance change after the thermal history with respect to the initial resistance value is small and that the characteristics are stable.
- the resistance value characteristics of the thermistor elements differ depending on the materials constituting the elements, and various materials exhibiting the resistance value characteristics according to the purpose of use have been developed.
- a thermistor element for detecting a high temperature range of about 100 ° C. such as an exhaust gas temperature for automobiles, a gas flame temperature of a gas water heater, a temperature of a heating furnace, etc.
- Perovskite-based materials such as those described in No. 1,528, are mainly used.
- Perovskite The system material is generally a composite oxide having a perovskite structure represented by (MM ') 03.
- oxides such as Y, Sr, Cr, Fe, and Ti are prescribed. It is described that a porcelain composition for a thermistor element, which was mixed at the following composition ratio and fired to obtain a complete solid solution, was used in a high temperature range and exhibited stable characteristics. Disclosure of the invention
- the conventional thermistor element described in the above publication is suitable for measurement in the medium to high temperature range of about 400 to 130 ° C, but is low in the temperature range of room temperature to about 400 ° C. Since the resistance value increases in the medium temperature range, there is a problem that it is not possible to determine the insulation and the temperature cannot be detected. On the other hand, it is possible to adjust the resistance value characteristics by changing the composition and substitution ratio of the composite perovskite oxide.
- the resistance value of the thermistor element is too low in the high temperature range, so that the desired resistance value range (100 Q to 100 kQ) cannot be satisfied, or thermal history, etc. It was found that there was a problem that the change in the resistance value due to the above was as large as about 10 to 30% and the stability was poor.
- the thermistor element To reduce damage to the co-fired lead wire material, the firing temperature should be lower, for example, an easily sinterable thermistor that can be fired at a temperature lower than 160 ° C. Evening elements are desired.
- the resistance value is in the range of 100 ⁇ to 100 k ⁇ in the temperature range of room temperature to 100 ° C., and the resistance value changes with respect to heat history and the like. It is a first object of the present invention to obtain a wide-range type thermistor element exhibiting both small resistance characteristics and low resistance value characteristics and resistance value stability. In addition, even at a high temperature of about 140 ° C. to 150 ° C., there is no change in resistance value, showing high heat resistance, or it can be easily fired at a temperature lower than 160 ° C. The second object is to obtain a thermistor element having excellent sinterability.
- the thermistor element according to claim 1 of the present invention is a mixed sintered body ( ⁇ ⁇ ) 0 of a composite perovskite oxide represented by ( ⁇ ⁇ ) 0 and a metal oxide represented by AC. 3 ⁇ ⁇ ⁇ ⁇ ⁇
- M is one or more elements selected from Group 2A elements of the periodic table and Group 3A elements excluding La
- M ′ is one or more elements selected from Group 3B, 4A, 5A, 6A, 7A and 8 elements of the periodic table
- the metal oxide AO x has a melting point of 130 ° C. or more, and the resistance value (100 ° C.) of A ⁇ alone in the thermistor element shape is 100 ⁇ or more. It is characterized by being a high resistance heat-resistant metal oxide.
- the conventional thermistor element with a bevelskite-type structure made of a complete solid solution can achieve both resistance characteristics in the temperature range from room temperature to 100 ° C and stability due to thermal history. Can not. Therefore, in the present invention, not a complete solid solution but a temperature range from room temperature to 100 ° C. Oite the composite base mouth Busukai gate oxide having a relatively low resistivity characteristics (MM ') 0 3, and Mochiiruko a mixed sintered body of high resistance and high heat resistance of the metal oxide A_ ⁇ Thus, a new thermistor element having both characteristics has been realized.
- the metal oxide AC has a high resistance value
- the resistance value of the composite perovskite oxide (MM ′) 0 in a high temperature range can be increased, and the melting point is high and the heat resistance is high. Because it is excellent, the high temperature stability of the thermistor element can be improved. Therefore, the resistance value in the temperature range of room temperature to 100 ° C. is in the range of 100 ⁇ to 100 k ⁇ , and the change in resistance value due to heat history and the like is small. It is possible to obtain a drain type thermistor element, which is suitably used for a temperature sensor or the like, and can exhibit high performance in a wide temperature range.
- the mole fraction of the composite perovskite oxide (MM ′) 0 in the mixed sintered body is a and the mole fraction of the metal oxide AC is b
- the above-mentioned effect can be achieved more reliably when the molar fractions a and b of the composite beta oxide (MM ′) 0 and the metal oxide AC have the above relationship. .
- M is Mg, Ca, Sr, Ba, Y, C e, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Yb and Sc, one or more elements selected from the group consisting of M ' A l, G a, T i, Z r, H f, V, N b, T a, C r, M o, W, M n, T c, R e, F e, C o, N i, R one or more selected from u, R h, P d, O s, Ir and P t It is practically preferable that the element be
- metal A in the metal oxide AO B, Mg, Si, Ca, Sc, Ti, Cr, Mn, Fe, Ni, Zn, Ga, Ge, Sr, Zr, Nb, Sn, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm , Yb, Lu, Hf, and Ta are used.
- cormorants good of claim 5 as the above metal oxide A_ ⁇ x, M G_ ⁇ , S i 0, S c 0 , T i 0, C r 2 ⁇ 3, M N_ ⁇ , M n 0, F e 2 0 3 , F e 3 ⁇ 4, n i ⁇ , Z N_ ⁇ , G a 2 0, Z r 0 2, n b 2 0, S n 0 2, C E_ ⁇ 2, P r 2 ⁇ 3, N d 0, S m 0, E u ⁇ , G d 2 0 3, T b 2 0 3, D y 0, H o 0, E r 2 0 3, T m 2 0 3, Y b 2 0 L
- One or more metal oxides selected from U 0, H f 0, and T a0 Each of these metal oxides has high resistance and high heat resistance, and contributes to the improvement of the performance of the thermistor element.
- the metal oxide AO a composite metal oxide containing one or more selected from Mg, Y, A 1 and Si can also be used.
- M g A l 2 0 , YS i 0, 3 A 1 2 0 ⁇ 2 S i 0, YA 1 0, YA 1 5 ⁇ l 2, 2 M g 0 ⁇ S i 0, C a S i 0 and M g C type no shiso is more composite metal oxide selected from the r ⁇ 4 and the like, both, the high resistance value Shows high heat resistance and contributes to the improvement of thermistor element performance.
- metal oxide AC MgO, Sc0, Z ⁇ 0, LU0, Hf0, C ⁇ 0, ⁇ ⁇ ⁇
- the C a 0, C a C 0 , S i ⁇ 2 and C a S i 0 3 sac Chino least one or as a sintering aid It can also be added.
- These sintering aids increase the sintering density of the mixed sintered body and improve element characteristics.
- An eleventh aspect of the present invention provides a temperature sensor comprising the thermistor element according to any one of the first to tenth aspects.
- the thermistor element having the structure of each of the above-mentioned claims can detect temperature over a wide temperature range and has stable characteristics, so that it is possible to realize a temperature sensor having high performance and excellent durability. it can.
- the invention of claim 12 is a method for producing the thermistor element according to any one of claims 1 to 10, wherein the composite solid bushing force oxide (MM ′) 0 a
- the above metal oxide ACU is mixed and pulverized, and the mixture after pulverization is adjusted to have an average particle diameter equal to or less than the average particle diameter of the above metal oxide A ⁇ before mixing, and then molded and fired into a predetermined shape. This is the feature.
- the variation of the temperature accuracy is, the composite base Robusukai preparative oxides obtained Ri by the calcination (MM ') 0 3 (or (MM' ) average particle size of 0 3 ⁇ a 0), but this and the larger Ri by an average particle size of the metal oxide AC to be mixed, the variation in composition of the mixed sintered body without both uniformly mixed, As a result, it was found that the resistance value of the thermistor element varied.
- the two are mixed, pulverized and atomized, and the average particle diameter is set to be equal to or less than the average particle diameter of the metal oxide A CU before mixing. It has been found that this composition variation can be reduced and the variation in resistance value can be reduced. Therefore, according to this method, a wide-range thermistor element with less variation in temperature accuracy can be realized.
- the raw material of M and the raw material of M 'in the composite perovskite oxide (MM') 03 are mixed and pulverized, and the average particle size of the mixture after pulverization is determined before mixing.
- the composite perovskite oxide (MM ') 03 was obtained, and this was used as the metal oxide. After mixing with the product A ⁇ , it is shaped into a predetermined shape and fired.
- the raw material of M and the raw material of M 'in the composite perovskite oxide (MM') 0 are mixed and pulverized, and the average particle size of the pulverized mixture is determined before mixing.
- the composite perovskite oxide (MM ') 0 was obtained.
- the vitreous bushing oxide (MM ') 0 and the above-mentioned metal oxide AO, are mixed and ground, and the average particle size of the mixture after milling is calculated as the average of the above-mentioned metal oxide A 0 before mixing. After reducing the particle size to below, it is shaped into a predetermined shape and fired.
- This method is a combination of the methods of claims 12 and 13 described above, and by combining the effects of both methods, a wide-range thermistor element with further reduced variation in temperature accuracy is provided. realizable.
- the thermistor element of the present invention is composed of a mixed sintered body obtained by mixing a composite perovskite oxide represented by (MM ′) 0 and a metal oxide represented by A 0 ⁇ and firing the mixture. And represented by the following general formula (1).
- a indicates the mole fraction of ( ⁇ ′)
- b indicates the mole fraction of A CU.
- ( ⁇ ′) 0 constituting the thermistor element of the present invention is a composite oxide having a belovskite structure, and ⁇ is selected from elements of Group 2A of the periodic table and Group 3A excluding La.
- M ' is selected from elements of Groups 3B, 4A, 5A, 6A, 7A and 8 of the Periodic Table. Indicates one or more elements.
- La has high hygroscopicity, and reacts with moisture in the air to form unstable hydroxides, which causes problems such as destruction of the thermistor element. Not used as M because of W.
- the elements of Group 2A that become M include, for example, Mg, Ca, Sr, and ⁇ a
- the elements of Group 3 include, for example, Y, C e, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Yb, Sc.
- a group 3B element that becomes M ′ for example, A 1 and Ga are listed
- a group 4A element for example, Ti, Zr, and Hf are listed as 5th
- Group V elements such as V, Nb, and Ta are group 6A elements; for example, Cr, Mo, and W are group 7A elements.
- M n, T c, and R e are group 8 elements, for example, F e, C o, N i, R u, R h, P d, O s, I r , Pt are preferably used.
- the combination of M and M ' can be arbitrarily combined so as to obtain a desired resistance value characteristic.
- the composite perovskite oxide (MM') 0 in which M and M 'are appropriately selected is The low resistance value and the low temperature coefficient of resistance (for example, 100 to 400 (K)) are shown.
- a complex perovskite oxide (MM ′) 0 for example, Y (Cr, Mn) 0 is preferably used.
- the molar ratio of each element can be appropriately set according to desired resistance value characteristics.
- a metal oxide AC is mixed and used as a material for stabilizing the resistance value of the thermistor element and keeping it in a desired range. Therefore, the characteristics required for the metal oxide AC include: (1) having a high resistance value in a high temperature range, and (2) being excellent in heat resistance and being stable at a high temperature. Specifically, for (1), a normal server used as a sensor In the dimensions of the mixing element, the resistance of AC alone (excluding the complex perovskite oxide) at 100 ° C should be 100 ⁇ or more.
- the temperature must be at least 1300 t and sufficiently higher than the sensor's normal maximum temperature of 10000 ° C.
- metal A in the metal oxide AO, B, M g, S i, C a, S c, T i, C r, M n, F e, N i, Z n, G a, G e, Sr, Zr, Nb, Sn, Ce, Pr, Nd, Sm, Eu, Gd, Tb, Dy, Ho, Er, Tm, Yb, Lu , H f, and Ta are preferably used.
- metal oxide AO x M g ⁇ , S i 0, S c 0, T i 0, Cr 2 ⁇ 3 , M n O, M n 0, F e 0, F e 3 0 4, n i ⁇ , Z n ⁇ , G a 2 0 3, Z r 0, n b 0, S n ⁇ 2, C e 0 2, P r 2 0 3, n d 2 0, S m 0 , E u 0, G d 2 0 3, T b 2 0 3, D y 2 0, H o 0, E r 0, T m 2 0 3, Y b 2 0 3, L u 2 0, H f 0 2.
- One or more gold oxides selected from T a0 can be used.
- the metal oxide A ⁇ a composite metal oxide containing one or more selected from Mg, ⁇ , A 1 and S i can be used. Specific examples of this include M g Al 20 , YS i 0, 3 A 10 ⁇ 2 S i 0, YA 10, Y 3 A 15 5 1 2 , 2 M g 0 ⁇ S i 0 , etc. C a S i 0 and M g C r ⁇ 4 and the like, also i'm on the Mochiiruko these sac Chino one or more of the complex metal oxide, the 1, to satisfy the characteristics of 2 be able to.
- Group 1 includes gold with a melting point of 2000 ° C or more. This is a group of oxides of the group AO, and has the effect of greatly improving the heat resistance of the thermistor element in addition to the above-mentioned effects (desired resistance characteristics and resistance stability).
- M g ⁇ , S c 0, Z r 0 , L u 0, H f 0 2 has a melting point as high as 2 4 0 0 ° C or more, the effect of improving the heat resistance of the thermistor element It is effective when used in an environment where it is constantly exposed to a high temperature of around 1000 ° C.
- Group 2 is a group of metal oxides A 0 having a melting point lower than 1000 t.
- the group of thermistor elements This has the effect of greatly improving sinterability.
- sintering can be performed at a temperature lower than 160 ° C., and there is an advantage that damage to the lead wire material due to sintering can be reduced. Also, the manufacturing cost can be reduced by lowering the firing temperature.
- a indicates the mole fraction of the composite oxide (MM ′)
- b indicates the mole fraction of the metal oxide AO, ing.
- the mixed sintered body can contain at least one of Ca ⁇ , CaC 0, Sio, and CaSio as a sintering aid.
- These sintering aids have the effect of forming a liquid phase at the firing temperature of the mixture of the composite oxide (MM ′) 0 and the metal oxide A O, and promoting sintering. Thereby, the sintering density of the obtained mixed sintered body is improved, the resistance value of the thermistor element is stabilized, and the variation in the resistance value with respect to the change in the firing temperature can be reduced.
- the addition amount of these sintering aids is appropriately adjusted according to the type.
- the element 1 and 2 show an example of a thermistor element 1 made of the mixed sintered body and a temperature sensor S using the same.
- the element 1 has a shape in which each end of two parallel lead wires 11 1 and 11 is embedded in the element section 13.
- the element is formed into, for example, a cylindrical shape having an outer diameter of 1.6 mm to form an element portion 13.
- This thermistor element 1 is incorporated into a general temperature sensor assembly shown in FIG.
- the temperature sensor S has a cylindrical heat-resistant metal case 2, and the thermistor element 1 is disposed in the left half thereof.
- One end of a metal pipe 3 extending from the outside is located in the right half of the metal case 2.
- the metal pipe 3 holds lead wires 31 and 32 inside as shown in FIG. 2 (b), and these lead wires 31 and 32 pass through the inside of the metal pipe 3.
- the lead wires 11 and 12 have, for example, a wire diameter of 0.
- the wire diameters and lengths of the lead wires 11 and 12 can be arbitrarily selected according to the shape and dimensions of the temperature sensor and the operating environment conditions of the temperature sensor.
- the material of the lead wires 11 and 12 is not limited to Pt100 (pure platinum) but also has a melting point that can withstand the sintering temperature of the thermistor element 1.
- a high melting point metal such as (platinum 80% iridium 20%) may be used.
- the cross-sectional shape is changed to a shape other than a circle, for example, a rectangle or a semicircle, or the lead wire 11 or 12 is knurled on the surface. It is also possible to provide irregularities by processing or the like.
- the basic manufacturing method (1) and the manufacturing methods (2) and (3), which are partially modified, are shown below.
- the manufacturing process is large and requires preliminary firing.
- the process is divided into a second preparation step for obtaining a thermistor element.
- the first preparation step first, powders of oxides (M ⁇ ,, M'0,) of these elements to be used as raw materials for M and M 'are prepared. Is prepared so as to have a desired composition (formulation (1) step). Next, water and the like are added to the mixture, mixed with a ball mill or the like (mixing step), dried with hot air, and roughly pulverized using a raikai machine or the like to obtain a mixed powder. The mixed powder is pre-fired to obtain a pre-fired body (MM ′) 0 3 (temporary firing step).
- the calcination temperature is usually 100 ⁇ ! It should be about 500 ° C.
- a binder may be added in the mixing step, and pre-baking may be performed using the mixed powder that has been granulated and dried using a spray drier.
- pre-baking may be performed using the mixed powder that has been granulated and dried using a spray drier.
- the above can also be implemented.
- Compounds other than oxides can also be used as raw materials for M and M '.
- the obtained calcined body and A 0 are blended in the molar fractions a and b such that the desired resistance value and the resistance temperature coefficient are obtained (the blending (2) step).
- This is granulated and dried using a spray drier (granulation / drying process), molded into a predetermined shape incorporating a lead wire made of Pt, etc. (molding process), and then fired.
- a thermistor element composed of the mixed sintered body ( ⁇ ⁇ ') 03 ⁇ A 0 is obtained.
- the firing temperature is usually about 1200 to 170 ° C., and a temperature at which the thermistor characteristics are most stable is appropriately selected.
- the lead wire can be formed by joining after firing.
- a binder, a resin material, or the like is mixed and added to the raw material of the thermal element, and the viscosity and hardness are adjusted to an appropriate value for the extrusion, and the lead is formed by extrusion.
- a molded body of a thermistor element having a hole formed therein is obtained, and a lead wire is loaded and baked, whereby a thermistor element having a lead wire formed thereon can be obtained.
- the thermistor element thus obtained is a mixed sintered body in which (MM ') 03, which is a perovskite compound, and the metal oxide AO, are uniformly mixed via the grain boundaries. ing.
- This thermistor element has a temperature range from room temperature (for example, 27 ° C) to about 1000 ° C.
- Low resistance value of 100 ⁇ to 100 k ⁇ required for W sensor, and resistance temperature coefficient ⁇ can be adjusted in the range of 200 to 400 (() Therefore, variation in resistance value due to temperature fluctuation can be reduced.
- the resistance change rate in the thermal history from room temperature to about 1000 ° C. can be stably realized at a level of about several percent.
- a wide-range thermistor element that can detect temperature in a wide temperature range from room temperature to 1000 ° C., has a small change in resistance due to heat history, and has stable characteristics. Furthermore, when the metal oxide A ⁇ of Group 1 is selected, high heat resistance that can withstand a high temperature of about 140 to 150 ° C. is obtained. When the oxide A ⁇ is selected, the sinterability is improved and firing at a temperature lower than 160 ° C. becomes possible.
- the first preparation step involves the step of preparing the raw material powders of M and M ′.
- a 0, which is an oxide of M, may be added in advance, mixed, and pre-fired to obtain a pre-fired body ( ⁇ ⁇ ') 0 ⁇ A 0.
- the calcined body was appropriately mixed with AC or the like so as to obtain a mixed sintered body having a desired molar ratio (a: b), and granulated and molded. Then, it is fired to obtain a mixed sintered body.
- the manufacturing method (2) is obtained by partially modifying the steps of the basic manufacturing method (1). That is, in this production method (2), in the second preparation step, in the step of mixing and pulverizing the calcined body and AC or the like, the average particle diameter of the mixture after pulverization is the average particle diameter of AC before mixing. Make sure that: As a specific means for atomizing the obtained mixture, a medium stirring mill or the like can be used. Is a grinding media include, for example Z r ⁇ 2 balls (0 0. About 5 mm) is used. Then, in the same way, the granulation, drying, molding, and firing steps are repeated. After that, it becomes a thermistor element.
- the temperature accuracy variation range (Soil A ° C) was ⁇ 20 to 30 ° C. ° C, the power is ok.
- observation of the material for the heat sink by SEM, EPMA, etc. revealed that the average particle size of the calcined product obtained in the first preparation step (for example, (MM ') 0, 2 to 5 m) is, in the case of the average particle size (e.g., D y 2 0 of a ⁇ to be mixed therewith, 1. 0 wm below) yo Ri also rather large, they do not uniformly mixed to this, mixed sintered
- the composition distribution of the body was found to vary.
- the mixture of the calcined body and AO, etc. is atomized in the mixing and pulverizing steps.
- the components are uniformly mixed, and the composition fluctuation of the mixed sintered body can be reduced.
- the variation in the resistance value of the thermistor element can be reduced.
- the variation width of the temperature accuracy (Soil A ° C) can be reduced to ⁇ 10 t or less. Therefore, in addition to the effect of the above-described manufacturing method (1), a better sensor temperature accuracy can be obtained. As shown in the figure (with little variation in temperature accuracy between sensors), a highly reliable wide-range thermostat can be obtained.
- the raw material of M' in the step of mixing the prepared raw material powders such as the oxide of M 'and the oxide of M in the first preparation step, the raw material of M' May be mixed and pulverized with the raw material of M so that the average particle size of the mixed and pulverized product is not more than the average particle size of the raw material of M before mixing and is 0.5 m or less. it can.
- the medium stirring mill used in the above-mentioned production method (2) can be used. Thereafter, calcining is performed in the same manner, and a second preparation process is performed to obtain a ceramic element.
- the mixing and pulverization steps in the prepared M ′ oxide may be pulverization using a normal ball mill or the like as in production method (1).
- a method of atomization using a medium stirring mill or the like as in the production method (2) may be adopted.
- uniform mixing of the calcined body with AC or the like is achieved in the subsequent steps (forming and firing steps) of the mixing and pulverizing steps in the second preparation step.
- the effect of the above manufacturing method (2) is provided, and the variation in the resistance value of the thermistor element can be reduced at a higher level.
- the temperature sensor using the thermistor element obtained by the above manufacturing methods (2) and (3) has a high temperature accuracy of 10 ° C or less because the temperature accuracy is suppressed to 10 ° C or less. It is suitably used for a required map control device, for example, a temperature monitor of an oxygen sensor for exhaust gas of an automobile.
- FIG. 1 is an overall schematic view of a thermistor element to which the present invention is applied;
- FIG. 2 (a) is an overall schematic view of a temperature sensor incorporating the thermistor element of the present invention;
- FIG. 2 (b) is a cross-sectional view thereof;
- FIG. 3 is a manufacturing process diagram of the thermistor device of Example 1 based on the manufacturing method (1) of the present invention:
- FIG. 4 shows a thermistor of Example 2 based on the production method (2) of the present invention. Evening element manufacturing process diagram
- FIG. 5 is a manufacturing process diagram of the thermistor element of Example 3 in which the manufacturing methods (2) and (3) of the present invention are combined;
- FIG. 6 is a view showing a manufacturing process of the thermistor element of Example 4 based on the manufacturing method (3) of the present invention
- FIG. 7 is a manufacturing process diagram of the thermistor device of Example 5 based on the manufacturing method (3) of the present invention.
- This manufacturing step corresponds to the above-mentioned manufacturing method (1), and includes a first preparation step of obtaining a calcined product of Y (Cr0.5Mn0.5) 03, from calcined product and D y 2 03 Metropolitan is divided into a second preparation step of obtaining a Sami scan evening element.
- a first preparation step first, as a starting material, either pure 9 9 9% more than Y 2 03, C r 2 03 and Micromax eta 2 0 3 powder was prepared, ⁇ :.
- C r Each was weighed so that the molar ratio of ⁇ was 2: 1: 1, and the total amount was 500 g (formulation (1) step).
- the average particle diameter of Y 2 03, C r 2 03 and M n 2 0 3 are respectively 0 U m N 2. 0 ⁇ 4. 0 m, it was 7. 0 ⁇ 1 5. O wm.
- the powder Y (C r 0. 5 M n 0. 5) 03 obtained in the first preparation step commercially available D y 2 0 3 powder ( A purity of 99.9% or more and an average particle size of 1.0 m were weighed so that the molar ratio became a predetermined ratio shown in Table 1, and the total amount was set to 500 g.
- the molar ratio is 36:64
- This mixed powder was used as a thermistor raw material to produce a thermistor element 1 having the same shape as that shown in FIG.
- the lead wires 11 and 12 are made of pure platinum (Pt100) with an outer diameter of 0.3 mm and a length of 10.5 mm, and are inserted with an outer diameter of 1.
- Pt100 pure platinum
- the molded body to be the element part 13 of the thermistor element 1 was then arranged in an A1203 corrugated mold set, and fired in air at 160 ° C. for 1 hour. In this way, mixed sintered body a Y (C r .. 5 Mn .. 5) 0 3 -. B D y 2 03 O Li Cheng OD 1 6 O to give mm of the thermistor element 1 (firing step ).
- the thermistor elements 1 of Examples 1, 1A, and 1B obtained in this manner and having different blending molar ratios (a: b) were respectively used in the general temperature sensor assembly shown in FIG. Temperature sensor S And
- ⁇ ( ⁇ ) 1 n (R / R.) / (1 / ⁇ — 1 / K.) ⁇ ⁇ ⁇ (2
- the rate of change in resistance indicates the change in resistance of the temperature sensor when each temperature sensor was subjected to a high-temperature endurance test for 100 hours at 110 ° C in air. It is represented by (3).
- R t is the initial resistance at a given temperature t (e.g., 500 ° C)
- R' t Indicates a resistance value at a predetermined temperature t after being left for 100 hours.
- the resistance value is in the range from 110 ⁇ to 100 k ⁇ , and the temperature coefficient of resistance ⁇ is 2 It is within a desirable range of 200 to 2480 0. It was also confirmed that the resistance change rate ⁇ R can be stably achieved at a level of about several percent.
- Table 2 also shows the results of evaluating the temperature accuracy of the temperature sensor incorporating the thermistor element of Example 1.
- the evaluation method was as follows. From the resistance-temperature data of many (for example, 100 units) temperature sensors manufactured in the same manner, a predetermined temperature (for example, 500 ° C.) The standard deviation ⁇ (sigma) of the resistance value is calculated. Six times the standard deviation ⁇ is used as the resistance value variation width (both sides), and the value obtained by halving the value obtained by converting the resistance value variation width into temperature is ⁇ . Then, it is written as temperature accuracy soil A t. Table 2 shows this A value, and as a result, the temperature accuracy of each sensor, A ° C, is ⁇ 23 ° C, and the variation range is a sufficiently practical value. I understood.
- a raw material in the same manner as in Example 1 Y 2 0 a, weighing C r 2 03 and Micromax eta 2 03 (the formulation (1) step), mixing by a ball mill (mixing step) And a mixed slurry was obtained.
- the average particle size is 1.
- ⁇ m Der Ri see Table 2
- the average particle size before mixing of D y 2 ⁇ 3 (teeth 0 m) Is also large.
- Y (Cr0.5Mn0.s) 03 powder average particle size 2-5 jum
- Dy 2 ⁇ 3 powder purity of 99.9% or more, average particle diameter of 1.0 m
- the molar ratio (a: b) becomes a predetermined ratio, and the total amount is .
- 2 0 0 0 g also as a sintering aid, 1 5 0 0 to 1 6 5 0 ° during firing (: a and a range of liquid phase becomes 5 1 ⁇ 2 and C a C_ ⁇ 3 used, the Y (C r .. 5 M n 0.
- This mixed and pulverized slurry was granulated and dried with a spray drier at a drying chamber inlet temperature of 200 ° C. and an outlet temperature of 120 ° C. (a granulating / drying step).
- the obtained granulated powder was spherical with an average particle diameter of 30 m.
- a thermistor element was formed in the same manner as in Example 1 (forming step). .
- Example 2 The thus-obtained summarizing elements of Examples 2, 2A, and 2B were further compared with Example 1 above.
- the sensor was incorporated into temperature sensors, and the temperature characteristics of the resistance value of each temperature sensor were evaluated.
- the results are also shown in Table 1.
- Table 2 also shows the results of evaluating the temperature accuracy of the thermistor element of Example 2.
- the thermistor elements of Examples 2, 2A, and 2B exhibited the same temperature value of resistance as those of Examples 1, 1A, and IB, respectively. It has a similar effect of the temperature coefficient of resistance.
- the temperature accuracy was ⁇ 23 ° C in Example 1 but was reduced to 10 ° C in Example 2 in this Example. It can be seen that the variation can be reduced by the example method.
- the mixed sintered body a Y (C r M n) ⁇ 3 ⁇ b D y 2 ⁇ 3 by Li Cheng mono- miss evening element having the same composition as in Example 1, different Prototype by method.
- Y (C r M n ) 0 and the molar ratio of D y 2 ⁇ 3 (a: b) 3 6: 6 4.
- a thermistor device having a molar ratio (a: b) of 95: 5 and 95: 5 was produced, and the devices were designated as Examples 3A and 3B, respectively.
- This manufacturing process is a combination of the above-described manufacturing method (2) and manufacturing method (3). In the mixing step in the first preparation step and the mixing and pulverization step in the second preparation step, both are used. Medium Use a stirring mill.
- a first preparation step was weighed Y 2 0 3, C r 0 and M n 2 0 3 as a raw material in the same manner as in Example 1, was mixed material the total amount 2 0 0 O g (Formulation ( 1) Process).
- this mixed raw material was atomized using a medium stirring mill.
- the medium stirring mill the same pearl milling apparatus as used in Example 2 above was used.
- 4.5 liters of distilled water as a dispersion medium, a binder, a release agent and a dispersant were added, and the mixture was mixed and pulverized for 10 hours (mixing step).
- the operating conditions were as follows: peripheral speed: 12 m / sec, rotation speed: 3110 rpm, polyvinyl alcohol (PVA) as a cylinder, 20 g per 20 to 36 g of mixed raw material did.
- PVA polyvinyl alcohol
- the average particle size was 0.3 m (see Table 2). It has an average particle size before mixing of Y 2 03 (1. 0 li m) yo Ri also rather small, and 0.5 ⁇ m by Ri small.
- the obtained raw material slurry was dried with a spray dryer under the conditions of a drying chamber inlet temperature of 200 ° C. and an outlet temperature of 120 ° C.
- the obtained raw material powder is spherical with an average particle diameter of 30 ⁇ m.
- This raw material powder is put into a crucible made of 99.3% A12 ⁇ 3, and is heated to 110 ⁇ Pre-baking was performed at 1300 for 1-2 hours (pre-baking step).
- the (C r., 5 M n 0.5) 03 which became a lump solid by calcination, was coarsely pulverized with a raikai machine and turned into powder through a # 30 mesh sieve.
- the resulting Y (C r .. 5 M n 0. 5) powder and D y 2 03 powder containing ⁇ 3 (average particle size 1. 0 wm) predetermined The weight was weighed so as to obtain the ratio, and the total amount was set to 2000 g. Further, as a sintering aid was added to S i 0 2 3 wt 0/0 6 0 g, C a C 03 to 4.5 wt 0/0 9 0 g (Formulation (2) Step ). This was atomized using a pearl mill as a medium stirring mill (mixing / grinding step). The mixing and pulverization conditions in this step are the same as those in the mixing step in the first preparation step.
- the average particle diameter was 0.3 m (see Table 2). It has an average particle size before mixing of D y 2 03 (1. 0 ⁇ m) yo Ri is small.
- Example 3 This mixed and pulverized slurry was granulated and dried by a spray dryer in the same manner as in Example 1 (a granulation / drying step), and then molded (formed). Sintering process) and fired to form a thermistor element (sintering process).
- the thus obtained thermistor elements of Examples 3, 3A and 3B were further incorporated in a temperature sensor in the same manner, and the temperature characteristics of the resistance value of each temperature sensor were evaluated. The results are shown in Table 1. Table 2 also shows the results of evaluating the temperature accuracy of the thermistor element of Example 3.
- the thermistor elements of Examples 3, 3A, and 3B exhibited the same temperature characteristics of resistance values as those of Examples 1, 1A, and IB, respectively.
- the same effect as that of each of the above embodiments can be obtained with respect to the temperature characteristic of the resistance value, and it is understood that the temperature characteristic of the resistance value depends on the blending molar ratio.
- the temperature accuracy in Example 2 was 10 ° C for soil, and the temperature accuracy in Example 3 was further reduced to ⁇ 5 ° C. It can be seen that the variation can be further reduced by the method of the embodiment.
- Example 1 Based on the manufacturing process shown in FIG. 6, a mixed sintered body of the same composition as in Example 1 a Y (C r 0. 5 M n 0. 5) 0 3 ⁇ b D y 2 0 3 by Li Cheng Sami scan evening Devices were prototyped in different ways. At this time, as shown in Table 1, Y (C r 0 5 M n 0 5..) 0 3 and D y 2 0 3 molar ratio of (a: b) 3 6: 6 4 and the (Example Four ) . Similarly, thermistor elements having a molar ratio (a: b) of 95: 5 and 95: 5 were produced, and the resulting elements were referred to as Examples 4A and 4B, respectively.
- This manufacturing process corresponds to the above-mentioned manufacturing method (3), and a medium stirring mill is used in the mixing process in the first preparation process. That is, the third embodiment is different from the third embodiment in that a ball mill is used instead of a medium stirring mill in the mixing and pulverization processes in the second preparation process.
- the first preparation process is the same as in Example 3 above.
- the raw materials are weighed (formulation (1) process), mixed and pulverized by a medium stirring mill (mixed). Step), pre-baked (pre-baking step). Also in this example, the results of evaluating the mixed and pulverized raw material slurry with a laser particle sizer were used.
- the average particle size is 0.3 m (see Table 2), which is smaller than the average particle size of Y 20 before mixing (1.0 wm) and smaller than 0.5 wm. Was confirmed.
- a second preparation step weighed Y a (C r .. 5 M n) 0 of the powder and D yz ⁇ powder (average particle size 1. 0 m) to a predetermined ratio, the total amount The weight was set to 2000 g (formulation (2) step), and the weighed product was mixed and pulverized using a ball mill.
- This mixed and pulverized slurry was granulated and dried by a spray dryer (granulation / drying step), molded (molding step), and fired to form a thermistor element (fired) in the same manner as in Example 1 above. Process).
- the thermistor elements of Examples 4, 4A, and 4B obtained in this manner were incorporated in a temperature sensor in the same manner, and the temperature characteristics of the resistance value of each temperature sensor were evaluated. The results are also shown in Table 1. did.
- Table 2 also shows the results of evaluating the temperature accuracy of the thermistor element of Example 4.
- the thermistor elements of Examples 4, 4A, and 4B exhibited the same temperature characteristics of resistance as those of Examples 1, 1A, and IB, respectively.
- the same effect as that of each of the above embodiments can be obtained with respect to the temperature characteristics of the resistance value. It can be seen that the properties depend on the blending molar ratio.
- the temperature accuracy of Example 3 was as good as 9 ° C in soil as shown in Table 2, and by performing atomization in the first preparation step, the temperature accuracy of Example 1 was ⁇ 10%. It can be seen that the variation can be reduced at 23 ° C.
- a ceramic element composed of a composite perovskite oxide Y (Cr 0.5 Mn 0.5) 03 and various metal oxides A ⁇ shown in Table 2 was prototyped. Is an AC, P r 2 03 (real ⁇ 5), S m 2 03 (Example 6), N d 2 03 (Example 7), was used M g 0 (Example 8), respectively.
- the production process of this example is basically the same as that of Example 3 above, and in the mixing step in the first preparation step and the mixing and pulverization step in the second preparation step, both use a medium stirring mill. The material is atomized.
- a first preparation step in the same manner as in Example 3 to obtain a powder of ⁇ (C r 0. 5 M na . 5) 03.
- the second preparation step in Formulation (2) extent E, except for using A ⁇ , the various metal oxides in place of D y 2 0 3 were the same as in Example 3.
- the molar ratio of the metal oxides and Y (C r .. 5 M n 0. 5) 03 is to indicate Suyo in Tables 4-7, mono in the same manner as in Example 3 Mister devices were manufactured (Examples 5 to 8).
- both P r 2 03 used as the starting material, S m 2 03, N dz 03, M g ⁇ is a purity 9 9.9% or more
- S m 2 0 3 was 1. 0 m
- N d 2 03 is 1. 0 m
- M g 0 is 2 m.
- Examples 5A to 8A, 5B to 8B were produced (Examples 5A to 8A, 5B to 8B).
- the temperature sensor thus obtained was incorporated into a temperature sensor, and its resistance-temperature characteristics were evaluated.
- the evaluation method was the same as in Example 1, and the results are shown in Tables 4 to 7.
- Tables 4 to 7 the thermistor elements of the above-described embodiments have substantially the same effect as the embodiment 3 with respect to the resistance-temperature characteristics.
- Table 2 shows the results of evaluating the temperature accuracy of each of the thermistor elements of Examples 5 to 8.
- the values in parentheses in the column of temperature accuracy in Table 2 indicate the thermistor in the same manner as in Example 1 above, in which both the first and second preparation steps use a ball mill for mixing. This is the temperature accuracy when an element is manufactured.
- the method of the present embodiment showed that the temperature accuracy variation (Sat) was as good as 5 ° C in all cases, and that the method of Example 1 was used. It can be seen that the variability is smaller than in the case of ( ⁇ 23 ° C (: ⁇ 25 ° C).
- Table 2 shows the average after the mixing step in the first preparation step. The particle diameter and the average particle diameter after the mixing and pulverizing steps in the second preparation step are also shown.
- Example 9 As shown in Table 2, as the metal oxide AC, using a composite metal oxide 3 A 1 2 03 ⁇ 2 S i 0 2 ( mullite g), in Example 5 the same like manner, Sami A prototype star element was manufactured. As shown in Table 8, the molar ratio of the composite Berobusukai gate oxide compound Y (C r .. 5 M n 0. 5) 03 (a: b) 3 9: 1 and so as, the process shown in FIG. 7 among, the second formulation of the preparation process (2) step except for using 3 a 1 2 03 ⁇ 2 S i 02 in place of the P r 2 03 is mono- mistakes in the same manner as in example 5 An evening element was fabricated. (Example 9).
- a thermistor element having a molar ratio (a: b) of 95: 5 and 95: 5 was produced, and the results were referred to as Examples 9A and 9B, respectively.
- 3 A 1 2 0 3 ⁇ 2 S i 0 2 used was a 9 9. have 9% pure, average particle diameter was 2 m.
- the obtained thermal element was incorporated into a temperature sensor, and its resistance-temperature characteristics were evaluated.
- the evaluation method was the same as in Example 1, and the results are shown in Table 8.
- the thermistor element of the present example has substantially the same effect as that of Example 3 with respect to the resistance-temperature characteristics.
- Table 1 shows the results of evaluating the temperature accuracy of the thermistor element of Example 9. According to the present example, the temperature accuracy showed an excellent value of 5 ° C for soil, and it can be seen that the variation was small.
- Example 10 ⁇ 3 ⁇ 15 ⁇ 12 (Example 11), M g A 1 2 ⁇ 3
- Example 1 2 (Example 1 2), were used Y 2 S i 0 5 (Example 1 3), respectively.
- thermoistor elements (a: b) were modified as shown in Tables 9 to 12 to produce thermistor elements, which were referred to as Examples 10A to 13A and 10B to 13B, respectively.
- the raw materials used all had a purity of 99.9% or more, and the average particle size was 1 to 3 / m.
- the obtained thermistor element was incorporated into a temperature sensor, and its resistance-temperature characteristics were evaluated.
- the evaluation method was the same as in Example 1, and the results are shown in Tables 9 to 12.
- the thermistor element according to the present embodiment has substantially the same effect as the third embodiment with respect to the resistance-temperature characteristic.
- all the examples showed good values of temperature accuracy of 5 ° C.
- Example 5-8 Based on the manufacturing process shown in FIG. 7, in the same manner as in Example 5-8, various illustrating a composite Berobusukai gate oxide compound Y (C r .. 5 M n .. 5) ⁇ 3, Table 1 3, 1 4 A thermistor element consisting of the metal oxide A 0, was fabricated.
- various metal oxides A ⁇ shown in Tables 13 and 14, were used, and these metal oxides and Y (C r. 5 M n 0. a)
- a thermoluminescent device was fabricated in the same manner as in Examples 5 to 8 except that the molar ratio of 03 was as shown in Tables 15 to 42, respectively. (Examples 14 to 41).
- Table 1314 shows the evaluation results of the temperature accuracy of each of the thermistor elements of Example 1441.
- the values shown in parentheses in the column of temperature accuracy in Table 1314 are thermistors in the same manner as in Example 1 above, using a ball mill for both mixing in the first preparation step and the second preparation step. This is the temperature accuracy when a star element is manufactured.
- the variation in temperature accuracy (A ° C) was ⁇ 5, which was a good value, and the value of Example 1 was good. It can be seen that the variation is smaller than that in the case of manufacturing by the method (2) ( ⁇ 23 ° C: up to 25 ° C).
- the average particle diameter after the mixing step and the average particle diameter after the mixing and pulverizing step in the second preparation step are also shown.
- a low resistance value and a low resistance temperature coefficient are provided.
- the resistance value and the temperature coefficient of resistance of the element can be controlled in desired ranges, and the characteristics can be stabilized. Therefore, it is possible to detect the temperature over a wide temperature range from room temperature to 1000 ° C, and there is no change in the resistance value due to the heat history from room temperature to 1000 ° C. This can greatly improve the reliability and durability of the temperature sensor.
- the thermistor raw material is atomized and the average particle diameter is controlled within a predetermined range, thereby achieving uniform mixing of the composition. Variations in temperature accuracy from room temperature to 1000 ° C. (at soil A) can be reduced to 10 ° C. or less, so that the temperature sensor can be made more accurate.
- Tables 43 to 45 show the firing temperatures of the thermistor elements and the heat resistance evaluation results in Examples 1 to 41 described above.
- Table 43 shows the group 1 having a higher melting point of 2400 ° C or higher
- Table 44 shows the group having a melting point of 20000 ° C or higher and lower than 2400 ° C.
- Table 45 shows those of Group 2 having a melting point lower than 2000 ° C.
- the firing temperature was the temperature at which the most stable resistance value characteristics were obtained in each of the thermistor compositions of Examples 1 to 41.
- the method of evaluating the heat resistance of the thermistor element is as follows.
- the thermistor element of each composition is placed in a high-temperature furnace, and the evaluation temperature (120 ° (:, 140 ° C, 15 ° C) (100 ° C.) for 100 hours, the resistance change rate of the device was measured, and evaluated according to the following criteria.
- Resistance change rate (%) ((resistance value after endurance / pre-endurance (initial) resistance value) )-1) x 1 0 0 Judgment standard :: Resistance change rate less than 5%
- Table 4 3 4 in earthenware pots by apparent to 4, melting point Sami scan evening element using 2 0 0 0 ° C or higher and a high metal oxide A 0 of group 1 x are both 1 5 0 0 °
- the resistance change rate is as high as less than 5% up to C, indicating excellent heat resistance.
- the higher the melting point of these metal oxides AO x the higher the heat resistance Is expected to be high, but the group in Table 43 with a melting point of 2400 ° C or higher has a slightly higher firing temperature of 1650 ° C, and in terms of energy cost,
- the groups in Table 44 which have lower temperatures of 1650 ° C to 1650 ° C, are more advantageous.
- the thermistor element using the metal oxide A 0: of Group 2 whose melting point is lower than 2000 t was obtained at 140 ° C. and 150 ° C.
- the rate of change of resistance at ° C is lower than that of Group 1
- the rate of change of resistance at 1200 ° C is less than 5% in all cases, and has sufficient heat resistance for practical use, and more than 1200 It can be fired at a relatively low temperature of 1150 t, and exhibits excellent sinterability. Therefore, when fabricating a thermistor element according to the present invention, the metal oxide AOx is used so that necessary characteristics can be obtained in consideration of the influence on the lead wire, the production cost, the use environment, and the like. You just have to select
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- Structural Engineering (AREA)
- Inorganic Chemistry (AREA)
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- General Life Sciences & Earth Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
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Abstract
L'invention concerne une unité de thermistance d'un dispositif à thermistance constitué d'un mélange de corps fritté (MM') O3 . AOx d'un composite d'oxyde de pérovskite représenté par (MM') O3 et un oxyde de métal représenté par AOx. M de (MM') O3 représentant au moins un élément choisi parmi les éléments du groupe 2A et ceux (sauf pour La) du groupe 3A dans la classification périodique, et M' représentant au moins un élément choisi parmi les éléments des groupes 3B, 4A, 5A, 6A, 7A, et 8 dans la classification périodique, et un oxyde de métal AOx utilisant un oxyde de métal à résistance thermique haute résistance présentant un point de fusion d'au moins 1300 °C et une résistance (1000 °C) de la substance AOx simple dans une forme de dispositif à thermistance d'au moins 1000Φ, présentant ainsi une résistance comprise entre 100Φ et 100k Φ dans un niveau de température de température ambiante de 1000 °C avec de faibles variations de température.
Priority Applications (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| EP00956821.3A EP1137016B1 (fr) | 1999-08-30 | 2000-08-30 | Dispositif a thermistance |
| US09/843,133 US20020020949A1 (en) | 1999-08-30 | 2001-04-27 | Thermistor element |
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP24294699 | 1999-08-30 | ||
| JP11/242946 | 1999-08-30 |
Related Child Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US09/843,133 Continuation US20020020949A1 (en) | 1999-08-30 | 2001-04-27 | Thermistor element |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| WO2001016966A1 true WO2001016966A1 (fr) | 2001-03-08 |
Family
ID=17096586
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| PCT/JP2000/005892 WO2001016966A1 (fr) | 1999-08-30 | 2000-08-30 | Dispositif a thermistance |
Country Status (3)
| Country | Link |
|---|---|
| US (1) | US20020020949A1 (fr) |
| EP (1) | EP1137016B1 (fr) |
| WO (1) | WO2001016966A1 (fr) |
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| JP2009173484A (ja) * | 2008-01-23 | 2009-08-06 | Mitsubishi Materials Corp | サーミスタ用金属酸化物焼結体及びサーミスタ素子並びにサーミスタ用金属酸化物焼結体の製造方法 |
| CN115894026A (zh) * | 2022-11-29 | 2023-04-04 | 唐山恭成科技有限公司 | 一种低电阻率高b值的ntc热敏电阻材料及制备方法 |
| CN116621579A (zh) * | 2023-05-24 | 2023-08-22 | 中国科学院新疆理化技术研究所 | 适用于宽温区测温的高精度热敏电阻材料及其制备方法 |
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| DE10239058A1 (de) * | 2001-08-27 | 2003-04-03 | Denso Corp | Verfahren zur Herstellung eines Heißleiterelements und Herstellungsgerät zur Herstellung von Rohmaterial für ein Heißleiterelement |
| WO2003042124A1 (fr) * | 2001-11-16 | 2003-05-22 | Ngk Spark Plug Co., Ltd. | Produit fritte pour element de thermistance et son procede d'elaboration, et detecteur de temperatures |
| EP1564197B1 (fr) * | 2002-11-18 | 2013-01-16 | NGK Spark Plug Co., Ltd. | Piece fritte pour element thermistance, son procede d'obtention, element thermistance et capteur de temperature |
| WO2006109792A1 (fr) * | 2005-04-11 | 2006-10-19 | Ngk Spark Plug Co., Ltd. | Oxyde fritte electroconducteur, element de thermistance utilisant cet oxyde fritte electroconducteur, et capteur de temperature utilisant cet element de thermistance |
| EP1876156B1 (fr) * | 2005-04-28 | 2014-12-10 | Murata Manufacturing Co., Ltd. | Composition ceramique piezoelectrique, procede de fabrication de ladite composition ceramique piezoelectrique, et composant electronique en ceramique piezoelectrique |
| JP5059332B2 (ja) * | 2006-02-16 | 2012-10-24 | 日本特殊陶業株式会社 | サーミスタ素子、これを用いた温度センサ、及びサーミスタ素子の製造方法 |
| JP2009249264A (ja) * | 2008-04-10 | 2009-10-29 | Sumitomo Chemical Co Ltd | 焼結体および熱電変換材料 |
| US9524814B2 (en) * | 2012-05-11 | 2016-12-20 | Industry-Academic Cooperation Foundation, Chosun University | Metal-oxide sintered body for temperature sensor, and method for manufacturing same |
| BR112015003594B1 (pt) * | 2012-08-20 | 2021-09-28 | Ceramtec Gmbh | Material compósito, emprego do material compósito e processo para produção de um corpo moldado sinterizado de um material compósito |
| JP6406022B2 (ja) * | 2015-01-13 | 2018-10-17 | 株式会社村田製作所 | Ｎｔｃサーミスタ素子の製造方法 |
| KR101908775B1 (ko) | 2015-04-06 | 2018-10-16 | 니뽄 도쿠슈 도교 가부시키가이샤 | 도전성 산화물 소결체, 그것을 사용한 서미스터 소자 및 온도 센서 |
| CN115036086A (zh) | 2018-10-31 | 2022-09-09 | 株式会社芝浦电子 | 热敏电阻烧结体及温度传感器元件 |
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| CN110931191A (zh) * | 2019-12-26 | 2020-03-27 | 广东爱晟电子科技有限公司 | Lu2O3稀土元素改性耐高温高可靠NTC半导体陶瓷热敏芯片材料 |
| CN111029069A (zh) * | 2019-12-26 | 2020-04-17 | 广东爱晟电子科技有限公司 | Tm2O3稀土元素改性耐高温高可靠NTC半导体陶瓷热敏芯片材料 |
| CN112830770B (zh) * | 2021-01-19 | 2023-03-21 | 中国科学院新疆理化技术研究所 | 一种高温复合热敏电阻材料及其制备方法 |
| CN117682842B (zh) * | 2023-12-14 | 2024-08-16 | 福建瑞升电子科技有限公司 | 一种ntc热敏电阻组合波瓷料及其制备方法 |
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| JPH08167502A (ja) * | 1994-12-13 | 1996-06-25 | Ooizumi Seisakusho:Kk | ガラス封止型サーミスタ |
| JPH1012405A (ja) * | 1996-06-24 | 1998-01-16 | Toyota Central Res & Dev Lab Inc | サーミスター用組成物 |
| EP0866472A2 (fr) * | 1997-03-19 | 1998-09-23 | Denso Corporation | Thermistor à large gamme de fonctionnement et son procédé de fabrication |
Family Cites Families (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| JP3254595B2 (ja) * | 1993-11-25 | 2002-02-12 | 日本特殊陶業株式会社 | サーミスタ用磁器組成物 |
| US5879750A (en) * | 1996-03-29 | 1999-03-09 | Denso Corporation | Method for manufacturing thermistor materials and thermistors |
-
2000
- 2000-08-30 WO PCT/JP2000/005892 patent/WO2001016966A1/fr active Application Filing
- 2000-08-30 EP EP00956821.3A patent/EP1137016B1/fr not_active Expired - Lifetime
-
2001
- 2001-04-27 US US09/843,133 patent/US20020020949A1/en not_active Abandoned
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH08167502A (ja) * | 1994-12-13 | 1996-06-25 | Ooizumi Seisakusho:Kk | ガラス封止型サーミスタ |
| JPH1012405A (ja) * | 1996-06-24 | 1998-01-16 | Toyota Central Res & Dev Lab Inc | サーミスター用組成物 |
| EP0866472A2 (fr) * | 1997-03-19 | 1998-09-23 | Denso Corporation | Thermistor à large gamme de fonctionnement et son procédé de fabrication |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2009173484A (ja) * | 2008-01-23 | 2009-08-06 | Mitsubishi Materials Corp | サーミスタ用金属酸化物焼結体及びサーミスタ素子並びにサーミスタ用金属酸化物焼結体の製造方法 |
| CN115894026A (zh) * | 2022-11-29 | 2023-04-04 | 唐山恭成科技有限公司 | 一种低电阻率高b值的ntc热敏电阻材料及制备方法 |
| CN115894026B (zh) * | 2022-11-29 | 2023-08-08 | 唐山恭成科技有限公司 | 一种低电阻率高b值的ntc热敏电阻材料及制备方法 |
| CN116621579A (zh) * | 2023-05-24 | 2023-08-22 | 中国科学院新疆理化技术研究所 | 适用于宽温区测温的高精度热敏电阻材料及其制备方法 |
Also Published As
| Publication number | Publication date |
|---|---|
| EP1137016A4 (fr) | 2008-03-19 |
| US20020020949A1 (en) | 2002-02-21 |
| EP1137016A1 (fr) | 2001-09-26 |
| EP1137016B1 (fr) | 2013-10-02 |
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